以天然鳞片石墨为原料,氧化插层制备可膨胀石墨,微波热解膨胀后,对膨胀石墨进行二次氧化插层并微波膨胀,采用超声剥离法制备出包含大量少层数碳原子的石墨烯纳米片.采用傅里叶红外光谱(FT-IR)、X射线衍射(XRD)、扫描电镜(SEM)、原子力显微镜(AFM)和拉曼光谱(Raman)对其结构和形貌进行分析.结果表明,氧化插层增大了石墨层间距,膨胀石墨更易于进一步氧化插层引入含氧基团；在微波作用下,石墨内部含氧基团热分解放出气体,进一步增大石墨层间距,甚至部分剥离；对二次膨胀处理的石墨薄片进行超声剥离可得到石墨烯纳米片,大部分石墨烯层数低于5层.
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